PMID- 20441225
OWN - NLM
STAT- MEDLINE
DCOM- 20100806
LR  - 20100505
IS  - 1520-5118 (Electronic)
IS  - 0021-8561 (Linking)
VI  - 58
IP  - 9
DP  - 2010 May 12
TI  - Multiresidue method for pesticides and persistent organic pollutants (POPs) in 
      milk and cream using comprehensive two-dimensional capillary gas 
      chromatography-time-of-flight mass spectrometry.
PG  - 5248-56
LID - 10.1021/jf100021p [doi]
AB  - A method for the analysis of pesticides and their metabolites including most of 
      the persistent organic pollutants (POPs) in milk and cream is described. The 
      method was single-laboratory validated through milk fortification in 
      quadruplicate with 34 pesticides, isomers, and metabolites including 12 of the 
      insecticide POPs and their metabolites. Whole cow's milk was fortified at 0.2, 
      0.4, 1, 2, 10, or 50 microg/kg wet weight and extracted with 
      acetone/cyclohexane/ethyl acetate (2:1:1) with the addition of Mg(2)SO(4) and 
      NaCl. Fat recovered in the extract accurately reflected the fat content of the 
      milk or cream. All test portions were purified on a gel permeation chromatograph 
      (GPC) followed by solid phase extraction (SPE) cleanup on a mixed bed graphitized 
      carbon black (GCB) and primary/secondary amine silica gel (PSA) column before 
      determination using a comprehensive two-dimensional gas chromatograph interfaced 
      to a time-of-flight mass spectrometer. Average recoveries were 77, 72, 73, 66, 
      77, and 84% for 0.2, 0.4, 1, 2, 10, and 50 microg/kg wet weight whole milk, 
      respectively. The average relative standard deviations for 0.2, 0.4, 1, 2, 10, 
      and 50 microg/kg were 10, 8, 7, 7, 3, and 3%, respectively. The limits of 
      quantification (LOQs) for all pesticides were 0.2 or 0.4 microg/kg wet weight. An 
      archived cream sample collected in 1982 on Oahu, Hawaii, was found to contain 
      only hepatachlor epoxide (HE) and DDE-p,p' at 380 +/- 24 and 69 +/- 17 microg/kg 
      fat, significantly elevated over the current action level of 50 microg/kg fat for 
      HE.
FAU - Hayward, Douglas G
AU  - Hayward DG
AD  - US Food and Drug Administration, College Park, Maryland 20740, USA.
FAU - Pisano, Tamani S
AU  - Pisano TS
FAU - Wong, Jon W
AU  - Wong JW
FAU - Scudder, Richard J
AU  - Scudder RJ
LA  - eng
PT  - Journal Article
PT  - Research Support, N.I.H., Extramural
PL  - United States
TA  - J Agric Food Chem
JT  - Journal of agricultural and food chemistry
JID - 0374755
RN  - 0 (Environmental Pollutants)
RN  - 0 (Pesticide Residues)
SB  - IM
MH  - Animals
MH  - Chromatography, Gel/*methods
MH  - Environmental Pollutants/*analysis
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Limit of Detection
MH  - Milk/*chemistry
MH  - Pesticide Residues/*analysis
EDAT- 2010/05/06 06:00
MHDA- 2010/08/07 06:00
CRDT- 2010/05/06 06:00
PHST- 2010/05/06 06:00 [entrez]
PHST- 2010/05/06 06:00 [pubmed]
PHST- 2010/08/07 06:00 [medline]
AID - 10.1021/jf100021p [doi]
PST - ppublish
SO  - J Agric Food Chem. 2010 May 12;58(9):5248-56. doi: 10.1021/jf100021p.